OFFICIAL REPORT OF BASICS CHEMICAL SEPARATION

POLYSULFONE (PSF) MEMBRANE MAKING

By:

ORISIA TORIQOTUL ULUM

22030194019

Chemistry Education 2022I

CHEMISTRY DEPARTMENT

FACULTY OF MATHEMATICS AND NATURAL SCIENCES

STATE UNIVERSITY OF SURABAYA

2023

I. Experiment Title
 Polysulfone (PSF) Membrane Making
II. Experiment Date
Thursday, November 16th, 2023 III.
Experiment Time
13.00-15.30 PM
IV. Experiment Purposes
1. To make polysulfone (PSF) membrane
2. Determine the thickness of the membrane
3. Determine the permeability value of the membrane
V. Basic Theory
5.1 Membrane

The membrane is a thin, semi-permeable layer that can pass

certain species and retain other species based on the size of the species
to be separated. The ability to control the permeation rate of different
chemical species is the main property of membranes which is the key
to widespread use of membranes (Baker, 2004).

The membrane structure can be homogeneous or

heterogeneous and can be thick or thin. The thickness and structure of
the membrane causes the membrane to have different functions and
can be adjusted to the needs of the separation process (Mulder, 1996).

5.2 Membrane Classification

5.2.1 Based on origin, membranes are divided into natural and
synthetic membranes. Natural membranes are usually made
from cellulose and its derivatives such as cellulose nitrate and
cellulose acetate. Meanwhile, examples of synthetic membranes
include polyamide, polysulfone and polycarbonate (Rautenbach
& Alberecht, 1989).
5.2.2 Based on the structure and separation principle, membranes can
be divided into:
a. Porous membrane
 This type of membrane has open or empty space, there are
various types of pores in the membrane. Separation using this
membrane is based on pore size. Selectivity is determined by
the relationship between pore size and the size of the particles
being separated. This type of membrane is usually used for
the separation of microfiltration and utrafiltration (Mulder,
1996).
b. Non-porous membranes
Non-porous membranes can be used to separate molecules of
the same size, both gases and liquids. Non-porous
membranes are thin layers with a pore size of less than 0.001
µm and low pore density. This membrane can separate very
small species that cannot be separated by porous membranes.
Non-porous membranes are used for gas separation and
pervaporation, the type of membrane can be a composite
membrane or asymmetric membrane, the separation is based
on solubility and differences in the diffusion speed of the
particles (Mulder, 1996).
c. Carrier Membrane
The mass transfer mechanism in this type of membrane is not
determined by the membrane (or the material of the
membrane) but is determined by specific carrier molecules
that make it easier for specific transfers to occur. There are
two concepts of the transfer mechanism of this type of
membrane, namely the carrier does not move in the
membrane matrix or the carrier moves when dissolved in a
liquid. The selectivity of a component is highly dependent on
the nature of the carrier molecule. High selectivity can be
achieved if a special carrier is used. The components to be
separated can be gas or liquid, ionic or non-ionic.
5.2.3 Based on pore geometry, membranes are divided into
asymmetric and symmetric
a. Symmetric membrane
 This membrane contains pores with a thickness of 10-200
µm. This membrane has a homogeneous pore structure
throughout the membrane. This type of membrane is less
effective because it allows pore blockages to occur more
quickly and results in fouling or pore blockage in the user
(Mulder, 1996).
b. Asymmetric membrane
This membrane consists of two layers, namely a thin and
dense skin with a thickness of 0.1-0.5 µm and a large porous
supporting layer with a thickness of 50-150 µm. Asymmetric
membranes produce higher selectivity due to the density of
the top layer of the membrane and have a high permeation
speed due to the thinness of the membrane. The high
filtration rate in this asymmetric membrane is due to the
surface filtration mechanism. The rejected particles are
retained on the membrane surface (Mulder, 1996).
5.2.4 Based on the operating system, they are divided into dead-end
and crossflow systems.

In cross-flow filtration, the feed is flowed perpendicular

to the membrane surface so that the particles accumulate and
form a layer on the membrane surface, this has an impact on
reducing flux and rejection. In the cross-flow type, the feed
flows along the membrane surface so that only part of it
accumulates.

5.2.5 Based on the pressure used as a force, membranes can be

classified into several types, namely: a. Microfiltration
Microfiltration (MF) membranes can be differentiated from
reverse osmosis (RO) and ultrafiltration (UF) membranes
based on the size of the particles they separate. In
microfiltration membranes, salts cannot be rejected by the
membrane. The filtration process can be carried out at
relatively low pressure, namely below 2 bar. Microfiltration
 membranes can be made from various kinds of materials,
both organic and inorganic. Inorganic membranes are widely
used because of their resistance to high temperatures.
Several techniques used to make membranes include
sintering, track atching, stretching, and phase inversion
(Wenten, 2000).
b. Ultrafiltration
The ultrafiltration process is between the nanofiltration and
microfiltration processes. Membrane pore sizes range from 1
µm to 1 nm. Ultrafiltration is used to separate
macromolecules and colloids from solutions. Ultrafiltration
and microfiltration membranes are porous membranes where
solute rejection is greatly influenced by the size and weight
of the solute relative to the membrane pore size. The size of
the molecules that can pass through the ultrafiltration
membrane ranges from 104-108 daltons (Mulder, 1996).
c. Reverse Osmosis
Reverse osmosis membranes (reverse osmosis) are used to
separate solutes that have a low molecular weight such as
inorganic salts or small organic molecules such as glucose
and sucrose from the solution. A denser membrane (smaller
pore size and lower surface porosity) with greater
hydrodynamic resistance is required in this process. This
causes the operating pressure in reverse osmosis to be very
large to produce the same flux as the microfiltration and
ultrafiltration processes. For this reason, in general, reverse
osmosis membranes have an asymmetric structure with a
thin and dense top layer and a supporting matrix 50-150 µm
thick. Resistance is determined by the tightness of the top
layer (Wenten, 2000).
5.3 Factors Affecting Membrane
Factors that influence the membrane separation process include a.
Membrane interaction with solution
 b. Pressure
c. Temperature, and
d. Concentration polarization
In use, membrane selection is based on the following properties: a.
Stable against temperature changes
b. Has resistance to chemicals
c. Ease of detecting leaks
e. Ease of replacement process
f. Separation efficiency

5.4 Types of Separation Applications with Membranes

According to Mulder (1996), there are 4 types of pushing

forces in separation using membranes. The performance of a
membrane installation depends on the type of thrust force used.
Various types of membrane separation applications based on the
driving force and installation performance include:

1. Pressure gradient driving force (ΔP)

Applications: microfiltration, ultrafiltration, nanofiltration, reverse
osmosis.
2. Concentration gradient driving force (ΔC)
Applications: pervaporation, gas permeation, vapor permeation,
dialysis, dialysis – diffusion.
3. Temperature gradient driving force (ΔT)
Application: thermo-osmosis, membrane distillation. Installation
performance is in the form of flux (J) and selectivity (α).
4. Electric Potential gradient driving force (ΔE)
Applications: electrodialysis, electro-osmosis, membrane-
electrolysis. The installation performance is in the form of flux (J)
and selectivity (α).
5.5 The Basic Material for Making Membranes
The basic material for making membranes is a polymer.
Various types of polymers have been widely used as materials for
making membranes. Commonly used polymers include polysulfone,
polyether sulfone, cellulose acetate, poly amide, poly ether ketone, and
so on.
There are many polymer additives for membrane
manufacturing, ranging from very expensive to cheap. The materials
used in the research include polysulfone (PSF) as a polymer,
Nmethylpyrrolidine (NMP) as a solvent, and zinc oxidation (ZnO) as
an additive. Polysulfone is a polymer that is often used as a basic
material in making membranes. This is because polysulfone has good
resistance to high temperatures, a wide pH range of 1-13, good
resistance to chlorine, and is easy to manufacture. Polysulfone is one
of the ultrafiltration membrane materials. Polysulfone membrane is a
membrane that is hydrophobic and has good mechanical properties,
has relatively large pores, so the water flow is also large. However,
this type of membrane has a weakness, namely that it is susceptible to
fouling. Fouling is the adhesion of unwanted particles during the
filtration process (Hartini & Syahbanu, 2018).

5.6 Membrane Working Principles

The separation process using membrane media can occur

because membranes have selectivity properties, namely the ability to
separate a particle from a mixture. This is because the particles have a
larger size than the membrane pores. For more details regarding the
separation process using a membrane, see the following image:
 Figure 1. Separation Scheme in Membranes (Mulder, 1996)

Feed consists of various molecules (components) that will. separated,

while downstream is the permeate side which is the result of
separation. Separation occurs due to a driving force so that the
molecules diffuse through the membrane due to the pressure
difference (∆P). concentration difference (∆C), energy difference
(∆E), temperature difference (∆T).

5.7 Membrane Manufacturing Techniques

Several techniques can be used to make synthetic membranes,

namely sintering, stretching, track-etching, template-leaching, coating
and phase inversion.

a. Sintering technique, which is a technique that produces porous

membranes (microfiltration) with a pore size of around 0.1-10 µm
which will produce porous organic and inorganic membranes.
Particles in the form of powder of a certain size are pressurized
and sintered at a certain temperature so that the interface of
adjacent particles disappears and new pores appear (Wenten,
2000).
b. Streching technique, which is a technique that produces pore sizes
of around 0.1–3 µm. The film made from semi-crystalline
polymer is pulled towards the direction of extrusion so that the
crystalline part of the polymer will be oriented parallel to the
direction of extrusion (Wenten, 2000).
c. Track-etching technique, which is a technique that produces pore
sizes of around 0.02–10 µm. The polymer film is shot with
highenergy radiation particles perpendicular to the direction of the
film so that it forms a trajectory in the polymer matrix and then
the film is put into a bath containing a non-solvent solution. The
pores produced from this technique are cylindrical in shape with
the same size and have a narrow pore distribution (Wenten, 2000).
d. Template-leaching technique, which is a way to release one of the
components (leaching) to create a porous membrane. This method
can be used to make porous glass membranes (Wenten, 2000).
e. Coating is a very simple method of making composite membranes
to obtain a very thin solid top layer. The methods used in making
this membrane are reverse osmosis, gas separation and
pervaporation. The principle of manufacture is by dipping the
asymmetric membrane into a coating solution containing polymer,
pre-polymer or monomer with a low solid concentration in the
solution (less than 1%). The asymmetric membrane is separated
from the bath containing the coating material and solvent to
obtain a thin layer of solution that adheres to the bath. The thin
layer is placed in an oven so that the solvent will evaporate and
crosslinking will occur (Mulder, 1996).
f. Phase Inversion Technique, which is a process of changing the
shape of a polymer from a liquid phase to a solid under controlled
conditions. The polymer solidification process begins with a
transition from liquid phase one to liquid phase two (liquid-liquid
demxing). At a certain stage during the demixing process, one of
the liquid phases (high concentration polymer phase) will solidify
to form a solid matrix.
 Figure 2. Phase Inversion Technique

Phase inversion techniques include precipitation methods with

controlled evaporation, precipitation with solvent evaporation, thermal
precipitation, vapor phase precipitation and immersion precipitation
(Mulder, 1996).

a. Precipitation by solvent evaporation Precipitation by solvent

evaporation is the simplest method, namely by dissolving the
polymer in a certain solvent and then printing it on a suitable
support to obtain a homogeneous membrane (Mulder, 1996).
b. Precipitation by controlled evaporation Precipitation by controlled
evaporation, namely dissolving the polymer in a mixture of
solvent and non-solvent. The solvent needed is a solvent that
evaporates more easily than a non-solvent, so that changes in
composition during evaporation will move towards increasing the
non-solvent content so that the polymer concentration becomes
more concentrated (Mulder, 1996).
c. Thermal precipitation Thermal precipitation accelerates phase
separation, so single solvents or mixed solvents are used. This
technique is usually used to manufacture microfiltration
membranes (Mulder, 1996).
d. Vapor phase precipitation Vapor consists of a saturated nonsolvent
and the same solvent, where the vapor atmosphere is placed as the
placement of the printed film. Vapor phase precipitation uses a
more concentrated solvent concentration so that the solvent does
not evaporate easily so that non-solvent penetration occurs into
the film (Mulder, 1996).
 e. Immersion precipitation Immersion precipitation, namely the
polymer solution is printed on a support and then immersed in a
coagulation bath containing a non-solvent. The structure of the
membrane formed is largely determined by a combination of mass
transfer and phase transfer (Mulder, 1996).

The requirement for making membranes using the phase inversion

method is that the polymer used must be soluble in the solvent or
mixture thereof. This condition is intended so that liquid liquid
demixing can occur. Demixing will occur in exchange of solvent with
non-solvent on the membrane. Withdrawing this solvent causes the
polymer to form a solid matrix and become a membrane. The
demixing process is divided into two mechanisms:

a. Instantaneous demixing Instantaneous demixing is demixing that

occurs immediately after the polymer is dipped into a coagulation
bath containing a non-solvent. The instantaneous demixing
mechanism that occurs forms a porous membrane (Wenten, 2000).
b. Delayed demixing Delayed demixing is demixing that occurs
when a polymer matrix is delayed before being dipped in a
coagulation bath. The membrane formed is a nonporous membrane
(Wenten, 2000).

5.8 Membrane Separation Process (Dead-End Principle)

Membranes as semi-permeable media must have good

performance. Factors that influence membrane performance are fairly
high selectivity and permeability, stability of mechanical properties,
stability to temperature and resistance to chemical substances. The
membrane separation process produces two streams, namely permeate
and retentate. Permeate is the result of separation that can pass through
the membrane, while retentate is the residual product that is retained
by the membrane (Pabby, Anil, Rizvi, & Sastre, 2009).
 Permeate and retentate are feed streams whose separation
process uses a dead-end or cross-flow filtration system (Mulder,
1996). Dead-end system, the feed solution is given a pressure push
force to pass through the membrane in a flow direction perpendicular
to the membrane. However, the weakness of this process is that it can
increase the retentate component in the feed solution by causing the
quality of the permeate to decrease. This is due to very high levels of
fouling due to the formation of a layer of particles on the membrane
surface. The thickness will continue to increase so that the flux value
decreases.

Figure 3. Dead-end filtration membrane system (Mulder, 1996)

5.9 Parameters That Influence Membrane Structure

The membrane formation mechanism is divided into two types,

namely porous membranes (microfiltration and ultrafiltration) and
nonporous membranes (dense), which is made using the phase
inversion method. Several parameters influence membrane
morphology (Mulder, 1996).

a. Selection of Solvent and Non-Solvent

The choice of solvent and non-solvent is one of the main variables
in the immersion precipitation process, the solvent and non-
solvent must dissolve each other. Generally, water is chosen as a
nonsolvent, although other non-solvents can be used, for example
HCl and NaOH as non-solvents in a coagulation bath.
Manufacture of polysulfone (PSF) membranes using N,N-
dimethylacetamide (DMAc) as a solvent and polyethylene glycol
 as an additive, with various non-solvent acids in a coagulation
bath solution.
b. Polymer Selection The choice of polymer is very influential
because the use of solvents or non-solvents in the inversion phase
is very limited. The choice of polymer will have an impact on
fouling and the temperature and chemical stability of the resulting
membrane. PAN, PSF and PES are types of polymers that can be
used to make ultrafiltration membranes with DMAc as a solvent,
the non-solvents are HCl, NaOH and water.
c. Polymer Concentration
An increase in the concentration of the casting solution will cause
an increase in the polymer concentration at the interface, resulting
in the resulting membrane having a smaller pore size and lower
flux.
d. Composition of the Coagulation Tank
The structure of the membrane formed will influence the addition
of solvent to the coagulation tank. The greater the solvent
concentration in the coagulation tank results in a decrease in the
polymer concentration at the interface, resulting in a membrane
with a larger pore size (Mulder, 1996).

5.10 Polymer

Polymer are long chain molecules formed by chemically

combining monomers through a process called polymerizaton. The
length of the polymer chain determines the degree of polymerization.
Polymers formed from two or more monomers that are called
copolymers. Copolymers are sometimes added in chain structures to
improve polymer properties (Karmakar, 1999). A polymer will form
when hundreds to thousands of small molecular units called
monomers bond together in a chain (Powel, 2003).
5.11 Polysulfone (PSF)

Polysulfone is a polymer that is often used as a basic material

in making membranes. This is because polysulfone has good
resistance to high temperature, a wide PH range of 1-13, good
resistance to chlorine, and is eary to manufacture. Polysulfone is one
of the Ultrafiltration membrone materials. Polysulfone membrane is a
membrane that is hydrophobic and has good mechanical properties,
has relatively large pores, so the water flow is also large. However,
this type of membrane has a weakness, that it is susceptible to fouling.
Fouling is the occurrence of unwanted particles sticking together
during the filtration process (Hartini & Syahbanu, 2018).

Polysulfone is a thermoplastic polymer with aryl -SO 2- aryl

subunits that is known for its high mechanical strength and stability at
high temperatures. Polysulfone has a molecular weight of around
35,000 with a repeating unit molecular weight of 442.52 g/mol,
containing sulfonate groups and a benzene core in a main polymer
chain. Polysulfone has properties that are hard, rigid, thermoplastic
and have a glass transition temperature (Tg) between 180ºC-250ºC.
The relative rigidity of the chain can be derived from the inflexibility
and immobility of the phenyl and sulfonyl groups, while the hardness
arises due to the presence of the ether group. Polysulfone is
hydrophobic because it has an aromatic group in its chemical
structure.

Figure 4. Structure of polysulfone polymer

5.12 N,N-dimethylacetamide (DMAc)

A solvent that has high solvent properties and is often used to

dissolve polysulfone polymers in making membranes. DMAc has the
 molecular formula C4H9NO, is a compound made from tris
(N,Ndimethyamine) phosphate and acetic acid anhydride which can
dissolve polysulfone well until a homogeneous solution is formed
(Stecher, Paul, & Thomas, 1960).

DMAc is hygroscopic and must be stored in an inert room,

does not evaporate easily and tends to be stable because it has a
relatively wide temperature resistance range with a boiling point
above 164,5166°C, a specific gravity of 0,937 kg/L, and a melting
point of -20°C. DMAc has a solubility parameter of 10,8 (cal/em),
dissolves in water and a polarity index of 6,8 (Bandrup , Immergut, &
Grulke, 1999).

5.13 Coagulation

A serious problem encountered in ultrafiltration membranes is

the tendency for flux to decrease throughout the operating time. This
can inhibit the subsequent separation of water that will pas through the
membrane (Rosenberg, et al., 2002). Therefore, processing is carried
out using a combination method of coagulation and ulrafiltration
membrane. Processing is preceded by a coagulation process followed
by an ultrafiltration process.

5.14 Flux
Flux is defined as the number of species that can penetrate the
membrane per unit area of the membrane per unit time. Flux is
determined by the number of membrane pores. Flux is expressed as
volume flux (J) which is expressed as follows (Mulder, 1996).

𝑉
J=
𝐴.𝑡

where:

J = flux volume (L.m-2.h-1)

 V = filtered volume (L) A

= membrane area (m2) t =

times (h)

VI. Tools and Materials

6.1 Tools
1. Beaker glass
2. Measuring cup
3. Volumetric flask
4. Watch glass
5. Drop pipette
6. Spatula
7. Funnel
8. Analytical balance
9. Magnetic stirrer
10. Casting knife
11. Coagulant bath
12. Screw micrometer
6.2 Materials
1. Polysulfone (PSF)
2. N,N-dimethylacetamide (DMAc)
3. Distilled water
VII. Experiment Flowchart 1. Preparation of molding solution

PSF and DMAc

1. Weighed in the ratio of 12/82

2. Dissolved using magnetic stirrer with 270 Rpm
C as long as 1 hour 15 minutes
3. Stirred in 60

Molding
Solution
2. Casting molding solution

Molding Solution

1.
Molds were made from glass with a thickness of 0.4 mm
and an area of 13x7 cm
2.
Molded using a casting knife with a pre-immersion time

Immersion stage precipitation casting molding solution

3. Preparation immersion stage

 Glass Plate

Put 1. into coagulation bath containing 1L Aquadest

2. With immersion temperature of 30C for 30 minutes

Immersed PSF Membrane

4. Washing Stage

Solid PSF Membrane

1.
Put into 500 mL aquadest tub for 1 minutes
2.
Repeated 2 times

Washed PSF Membrane

5. Drying stage

Washed PSf Membrane

1. Dried in room temperature 24 hours

Dried PSF Membrane

6. Permeabilty test

Glass Plate

1. Measured with a screw micrometer at 3 points

2. Average the thickness
3. Cut into a circle with a diameter of

4. Tested with a dead-end reactor using aquadest as feed

solution
5. Flux value obtained

Flux Value
Flux value formula:

𝑉
J=
𝐴.𝑡

where:

J = flux volume (L.m-2.h-1)

V = filtered volume (L) A

= membrane area (m2) t =

times (h)
VIII. Observation Results
No. Experiment Flowchart Experiment Result Alleged/Reaction Conclusion

Before After
1. Making Printing Solution - PSF = white - Molding PSF and DMAc
solid solution = dissolved completely
PSF and DMAc - DMAc = clear solution in 1 hour 30 minutes
and +
colorless homogeneous
1. Weighed by comparison
solution C4H9NO
(% b/b) (12/88)
- PSF = 1 gr ➔
2. Dissolved with a magnetig
- DMAc = 7,3
stirrer at speed of 270 rpm gr
3. Stirred at 60° C for an
hour

Molding solution
2. Casting Molding Solution - Mold from - Casting Membran printing
glass plate molding with a casting knife
Molding Solution with a with a thickness of 0,4
thickness of solution nm and an area 91
0,4 nm and - Inversed = cm2.
1. A mold is made from a an area of solution to
glass plate with a 91 cm2 (13 solid phase
thickness of 0,4 nm and cm x 7 cm)
an area 91 cm2 (13 cm x 7
cm)
2. Printend using a casting
knife with a pre
immursian time of 5
minutes

Stage immersion precipitate

casting solution
3. Precipitation Immersion Stage - Casting wet - Immersed PSF Precipitation occurs
molding membrane = due to the exchange of
solution white solvent and non
Place in a coagulation
Glass plate
bath containing 100 ml of solvent.
1. distillated water
With an immersion
temperature of 30° C for
2. minutes

30

Immersion PSF membrane

4. Washing Stage - White solid - Clean PSF The solid PSf

PSF membrane = membrane was
Solid PSF membrane membrane (washed) obtained clean from
= unwashed the remaining DMAc
solution that was still
1. Put into 500 ml attached.

distilled water both for a

minute
2. Repeated 2 times

Washed PSF membrane

5. Drying Stage - Clean PSF - Dry PSF Dry PSf membrane
membrane membrane ready for thickness
Washed PSF membrane test.
(washed)
still wet
1. Dried of room temperature
for ± 24 hours

Dried PSF membrane

6. Permeability Test
Dried PSF membrane
1. Measured with 5-
point screw micrometer
Measured the average
thickness
3. Cut into a circle with a
diameter of 6,3 cm
4. Tested with a dead-end
reactor using distilled
water feed solution
5. Obtained the flux value
Flux value
- Dry PSF The shape of the
membrane membrane is rectangle
with thickness of the
membrane are
- Spot 1 = 0,835 nm
2.
- Spot 2 = 0,429 nm
- Spot 3 = 0,270 nm
- Spot 4 = 0,618 nm
- Spot 5 = 0,580 nm
Average = 0,546 nm
Flux value
- 0,4 mm = 649,
350 L/m2 h
- 0,6 mm = 405,
844 L/m2 h
- 0,8 mm = 196,
772 L/m2 h
IX. Analysis

The experiment entitled “Polysulfone (PSF) Membrane Making”

which was held on Thursday, November 16th, 2023 at 13.00-15.30 PM aims
to make polysulfone (PSF) membrane, determine the thickness of the
membrane, and determine the permeability value of the membrane.

The reason polysulfone was chosen is because it has several

advantages, including thermal resistance, stability between pH 1-14,
stiffness, transparency, insoluble or damaged by dilute acids or alkalis, and
high mechanical strength. Polysulfone has hard, rigid, thermoplastic
properties and has a glass transition temperature (Tg) between 180ºC-250ºC.
The relative rigidity of the chain can be derived from the inflexibility and
immobility of the phenyl and sulfonyl groups, while the hardness arises due
to the presence of the ether group.

Meanwhile, the reason for choosing DMAc as a solvent is because

DMAc is difficult to evaporate with a high boiling point of 166ºC and has a
specific gravity of 0.94 kg/L so it can dissolve polysulfone well. To
determine the solvent is to choose a solvent with close solubility parameters.
The solubility parameters of DMAc are close to polysulfone.

9.1 Molding Solution Making

The first step is to weigh PSF and DMAc with a wt/wt ratio of 18/82
(1 g PSF and 7.3 g DMAc). The function of wt/wt percent is to assist
in regulating the composition and physical properties of the resulting
membrane. For example, by changing the weight percentage of a
material in a mixture, we can control the thickness, strength,
permeability, and other properties of the membrane to be printed.
Second, dissolved with a magnetic stirrer at a speed of 270 rpm and a
temperature of 60ºC until homogeneous. PSF and DMAc are
homogenized at a temperature of 60ºC because if it is above 60ºC the
DMAc will quickly evaporate, and if it is done below a temperature of
60ºC the PSF polymer bonds will not be broken. Stirring speed, time
and temperature influence the homogeneity of the molding solution
 formed and homogeneity will influence the shape of the membrane.
The higher the polymer concentration causes the membrane to have an
asymmetrical shape. After that, a colorless and homogeneous molding
solution will be obtained.
9.2 Casting Molding Solution
The first step is to create a border on the plate with a thickness of 0.4
nm with a size of 13 cm × 7 cm. The function of providing boundaries
is so that the printed membrane is evenly thin (flatsheet) and so that
there is no difference in thickness on each side of the printed
membrane. Second, printed using a casting knife with a pre-immersion
time of 5 minutes. The purpose of the pre-immersion time of 5
minutes before printing is to minimize the presence of bubbles.
Bubbles can create defects in the membrane. Membranes that have
defects will form large pores or often referred to as gaping holes
(makcrovoid). Meanwhile, the purpose of pre-immersion when
printing on a casting knife is to level it according to the column or
plate that has been made according to the thickness and area size of
the mold.
9.3 Precipitation Immersion Stage
The step is to place the plate in a coagulation bath containing 1000 mL
distilled water with an immersion temperature of 30ºC for 30 minutes.
The purpose of this step is to change the solid particles in raw water
that cannot settle into ones that are easy to evaporate. After being
placed in a coagulation bath, leave it for 30 minutes to produce a
white immersion PSF membrane. After the plate is placed in the
coagulant bath, the membrane becomes increasingly compact due to
the exchange between solvent and non-solvent (phase inversion).
Precipitation occurs due to the exchange of solvents and non-solvents,
where the hydrophobic membrane material when placed in water will
solidify.
9.4 Washing Stage
The step is to put the solid PSF membrane into 500 mL distilled water
bath for a minute and repeated 2 times. The purpose of washing is to
 remove solvents on the membrane surface. And the aim of repeating
this process is to produce a sample that is truly clean so that there are
no contaminating substances that could interfere with subsequent
experiments and to remove impurities that can clog the membrane
pores.
9.5 Drying Stage
The washed PSF membrane is dried at room temperature for 24 hours.
The goal is for the membrane to dry completely.
9.6 Thickness Test
The dried membrane is measured with a 5-point screw micrometer.
Membranes should not be measured before drying because this can
cause physical defects in the membrane. In addition, measurements
use 5-points to represent the average membrane thickness. From the
experiments that have been carried out, the membrane thickness is
obtained as follows:
a) Point 1 (middle point)
Fixed scale = 0,5 mm × 1 mm = 0,5 mm
Nonius scale = 33,5 mm × 0,01 mm = 0,335 mm
Result = fixed scale + nonius scale
= 0,5 mm + 0,335 mm = 0,835 mm
b) Point 2
Fixed scale = 0,1 mm × 1 mm = 0,1 mm
Nonius scale = 32,9 mm × 0,01 mm = 0,329 mm
Result = fixed scale + nonius scale
= 0,1 mm + 0,329 mm = 0,429 mm
c) Point 3
Fixed scale = 0 mm × 1 mm = 0 mm
Nonius scale = 27 mm × 0,01 mm = 0,270 mm
Result = fixed scale + nonius scale
= 0 mm + 0,270 mm = 0,270 mm
d) Point 4
Fixed scale = 0,2 mm × 1 mm = 0,2 mm
 Nonius scale = 41,8 mm × 0,01 mm = 0,418 mm
Result = fixed scale + nonius scale
= 0,2 mm + 0,418 mm = 0,618 mm
e) Point 5
Fixed scale = 0,1 mm × 1 mm = 0,1 mm
Nonius scale = 48 mm × 0,01 mm = 0,480 mm
Result = fixed scale + nonius scale
= 0,1 mm + 0,480 mm = 0,580 mm

➢ Average Thickness = 0,546 mm 5

0,835+0,429+0,270+0,618+0,580

9.7 Permeability Test

In this experiment, the step taken was that a dry PSF
membrane with a diameter of 7 cm with a thickness of 0.4 mm, 0.6
mm, and 0.8 mm was tested with a dead-end reactor using a 100-ppm
methylene blue solution in 250 mL. On a membrane thickness of 0.4
mm, it takes 350 seconds. On a membrane thickness of 0.6 mm, it
takes 600 seconds. On a membrane thickness of 0.8 mm, it takes 1200
seconds. After that, the flux value (J) can be calculated according to
the following formula:
𝑉
J=
𝐴.𝑡

where:

J = flux volume (L.m-2.h-1)

V = filtered volume (L) A

= membrane area (m2) t =

times (h)

Therefore, the flux value obtained is as follows: a.

0,4 mm with separation time 350 s = 0,1 h
b. 0,6 mm with separation time 600 s = 0,16 h
c. 0,8 mm with separation time 1200 s = 0,33 h
with a diameter of 7 cm. If the surface area is known as A = π (𝑑)2
2

J=𝑉

𝐴.𝑡

A = π (𝑑)2 = 22 (7)2
2 7 2

𝑉
a. J =
𝐴.𝑡

=
= 649,350 L/m2 h
𝑉
b. J =
𝐴.𝑡

=
= 405,844 L/m2 h
𝑉
c. J =
𝐴.𝑡

=
= 196,772 L/m2 h

The membrane performance evaluated is in the form of

permeability values expressed in flux. Membrane performance is
influenced by the size and distribution of the pores formed on the
membrane, the thicker the membrane, the smaller and fewer the pores
formed.
 The relationship between pore size and permeability is that if
the pore size is large, the membrane permeability is high, and vice
versa. Then the relationship between permeability and porosity is that
increasing porosity will be followed by increasing permeability.

9.8 Graphic Relationship between Membrane Thickness and Flux

Value

Relationship between Membrane Thickness and

Flux Value
Membrane Thickness
0.9 0.8
0.8
0.7 0.6
0.6
0.5 0.4
0.4
0.3
0.2
0.1
0
649,350 405,855 196,772
Flux Value

From the graph above, it can be concluded that the thicker the
membrane, the smaller the flux value. This means that the flux value is
inversely proportional to the membrane thickness. This is because the
thicker the membrane, the more resistance substances must overcome to
pass through the membrane. As a result, the amount of substances passing
through the membrane becomes less.
Apart from membrane thickness, the flux value is also influenced by
several other factors, such as the pressure difference between the two sides
of the membrane, concentration gradient, and membrane permeability. The
pressure difference between the two sides of the membrane causes
substances to move from the side with high pressure to the side with low
 pressure. A concentration gradient causes substances to move from the side
with high concentration to the side with low concentration. Membrane
permeability is a measure of how easily substances can pass through the
membrane. The greater the pressure difference between the two sides of the
membrane, the greater the concentration gradient, and the higher the
membrane permeability, the greater the flux value.

The decrease in membrane pore size along with the decrease in the
printed thickness of the psf membrane is due to the suppression or
minimization of macrofoites. Increasing the printing thickness tends to
lengthen the distance the solution travels through the membrane, resulting in
a decrease in the flow rate of the feed solution through the membrane.

X. Conclusion
From the experiment that has been done, it can be conclude:
1. One of the materials that can be used to make membranes is
polysulfone
(PSF) with DMAc solvent
2. The thickness of the membrane obtained:
a. Point 1 (middle point) = 0,835 mm
b. Point 2 = 0,429 mm
c. Point 3 = 0,270 mm
d. Point 4 = 0,618 mm
e. Point 5 = 0,580 mm
The average thickness is 0,546 mm
3. From the permeability test, the flux value is obtained:
a. 0.4 mm = 649,350 L/m2h
b. 0.6 mm = 405,844 L/m2h
c. 0.8 mm = 196,772 L/m2h

XI. Advices
In carrying out this practicum, you should first read and understand the
basic theory regarding the manufacture of polysuflon membranes (PSF).
 Then during the practicum, the practitioner must be more patient and careful
in weighing, measuring, observing and calculating in this Polysuflon
Membrane (PSF) Making experiment. This needs to be paid attention to
because if you are not careful it will affect the results of the membrane size,
flux value and rejection value during the physical test (thickness),
permeability test and membrane selectivity test.

XII. References

Baker, R. W. (2004). Membrane Technology and Application, 2nd Ed.

Chichester: John Wiley & Sons, Ltd.

Bandrup , J., Immergut, E. H., & Grulke, E. A. (1999). Polymer Handbook,

2nd Ed. New York: John Wiley & Sons, Interscience Publisher.

Hartini, A. S., & Syahbanu, I. (2018). Uji Water Uptake dan Porositas
Terhadap Blend Membran Berbasis Polisulfon dan Selulosa Asetat
dari Nata de Coco. Kimia Khatulistiwa, 7(4), 25-30.

Karmakar, S. R. (1999). Chemical Technology in the Pre-Treatment Process

of Textiles. New Delhi: Elsevier.

Mulder, M. (1996). Basic Principle of Membrane Technology. Netherlands:

Kluwer Academic Publisher.

Pabby, Anil, K., Rizvi, S., & Sastre, A. (2009). Handbook of Membrane
Separations Chemical, Pharmaceutical, Food, and
Biotechnological Applications. New York: CRC Press Taylor &
Francis Group.

Powel. (2003). Kejuruteraan dengan Polimer. Johor Baharu: University

Teknologi Malaysia.

Rautenbach, R., & Alberecht, L. (1989). Membrane Processe. USA: John

Wiley & Sons, Inc.

Rosenberg, U., Krugera, R., Witzigb, W., Manzb, U., Szewzykb, M., &
Krumea. (2002). Performance of Bioreactor with Submerge
 Membranes for Aerobic Treatment of Municipal Waste Water.
Water Research, 36, 413-420.

Stecher, P., Paul, G., & Thomas, A. (1960). The Merck Index of Chemical
and Drugs, 7th Ed. USA: Merck and Co Inc.

Wenten, I. G. (2000). Teknologi Membran Industrial. Bandung: Teknik

Kimia ITB.

XIII. Attachments a. Questions

4. Explain the advantages and disadvantages of polysulfone
membranes Answer:
Polysulfone membranes have high pH resistance and good
thermal stability. The advantages of polysulfone are that it is
resistant to extreme degrees of acidity, dissolves easily in
chloroform and dimethylformamide, and is easy to apply in
conventional processes. The disadvantages of polysulfone are that
it has high solubility, can only dissolve in organic solvents and is
hydrophobic
5. Explain the method used in the process of making polysulfone
membranes above!
Answer:
The membrane manufacturing method used in this study is the
phase inversion method which includes immersion precipitation
technique. Phase inversion is a process of changing the form of a
polymer from a liquid phase to a solid under controlled
conditions. This compaction process begins with the transition
from a single liquid phase to a liquid phase (liquid-liquid
demixing). At a certain stage during the demixing process, one of
the liquid phases (high concentration polymer phase) will solidify
to form a solid matrix. Controlling the initial stages of the phase
transition will determine the resulting membrane morphology.
The polymer solution after being printed is then dipped into a
coagulation bath containing nonsolvent. The membrane structure
is determined by a combination of mass transfer and phase
 separation. All phase inversion processes are based on the same
thermodynamic principles. The phase inversion technique has
several advantages including being easy to perform, pore
formation can be controlled and can be used on a variety of
polymers. Phase inversion is a process of changing the form of a
polymer from a liquid phase to a solid under controlled
conditions. The choice of solventnon-solvent system greatly
affects the resulting membrane structure. The non-solvent used as
a coagulant must be soluble in the solvent. Aquadest is a common
non-solvent used in phase inversion processes. The mixing
process can take place perfectly if the composition of all the
materials making up the membrane has the same solubility. In
addition, the total composition greatly determines the
homogeneity and performance of the membrane. The solubility of
polymers decreases with increasing molecular mass. If a polymer
is soluble in a suitable solvent and then a non-solvent is added (if
the polymer solution is poured into an excessive amount of the
non-solvent) the polymer will precipitate.
6. Explain the characteristics of a good membrane in terms of what?
Answer:
A good membrane has a good permeability and selectivity. The
permeability of a membrane is a measure of the speed at which a
species or constituent penetrates the membrane. In terms of
quantity, membrane permeability is often expressed as flux or
permeability coefficient. Then the selectivity of a membrane is a
measure of the ability of a membrane to retain a species or pass a
particular species. The parameter used to describe the membrane
permselectivity is the rejection coefficient (R). Besides that, a
good membrane has high thermal resistance and good chemical
resistance to extreme pH ranges